WO2023108378A1 - Fibre d'aérogel présentant une caractéristique morphologique de section spécifique, procédé et dispositif de préparation associés - Google Patents

Fibre d'aérogel présentant une caractéristique morphologique de section spécifique, procédé et dispositif de préparation associés Download PDF

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Publication number
WO2023108378A1
WO2023108378A1 PCT/CN2021/137642 CN2021137642W WO2023108378A1 WO 2023108378 A1 WO2023108378 A1 WO 2023108378A1 CN 2021137642 W CN2021137642 W CN 2021137642W WO 2023108378 A1 WO2023108378 A1 WO 2023108378A1
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Prior art keywords
fiber
graphene
graphene oxide
dimensional
nanosheets
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PCT/CN2021/137642
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English (en)
Chinese (zh)
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高超
李鹏
刘英军
许震
王子秋
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浙江大学
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Priority to PCT/CN2021/137642 priority Critical patent/WO2023108378A1/fr
Priority to JP2023574187A priority patent/JP2024520603A/ja
Publication of WO2023108378A1 publication Critical patent/WO2023108378A1/fr
Priority to US18/434,741 priority patent/US20240175169A1/en

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02—Heat treatment
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06—Washing or drying
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D13/00—Complete machines for producing artificial threads
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/04—Dry spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
    • D01D5/247—Discontinuous hollow structure or microporous structure
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00—Inorganic fibres
    • D10B2101/10—Inorganic fibres based on non-oxides other than metals
    • D10B2101/12—Carbon; Pitch
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/08—Physical properties foamed
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/16—Physical properties antistatic; conductive

Definitions

  • the invention relates to the field of nanomaterials, in particular to an airgel fiber with specific cross-sectional shape characteristics and a preparation method and device thereof.
  • Airgel fiber is an emerging material that combines the excellent properties of airgel and fiber. It refers to the gel fiber prepared by wet spinning through freeze-drying or normal pressure drying. Fiber varieties with high specific surface area and high porosity.
  • a two-dimensional sheet molecule is a molecule with a huge aspect ratio with a monoatomic layer thickness. Taking graphene as an example, it has extremely high tensile strength, Young's modulus, high electrical conductivity, and room temperature the highest thermal conductivity. In addition to typical high porosity and other characteristics, airgel fibers prepared with two-dimensional sheet-like molecules have more excellent mechanical-electrical-thermal properties.
  • the arrangement shape will also affect the effective transmission of electrons and phonons between the two-dimensional nanosheets with high electrical and thermal conductivity, and affect the conductivity of airgel fibers. Therefore, finding a strategy to effectively and precisely control the order of the two-dimensional sheet arrangement inside the airgel fiber has become a major research direction.
  • airgel fibers with specific cross-sectional morphological characteristics can be prepared, thereby promoting the practical application of airgel fibers.
  • the Gaochao Research Group of Zhejiang University invented a macroscopic graphene fiber with single-layer graphene as the assembly unit, creating a new way to prepare carbon fiber from natural graphite.
  • pure graphene fiber shows excellent characteristics in terms of thermal conductivity, which is much higher than that of traditional carbon fiber.
  • the mechanical properties of graphene fiber are mediocre.
  • its single-filament mechanical strength can reach 3.4GPa
  • its modulus has not yet reached Breaking through 400GPa is inconsistent with the law that the modulus and thermal conductivity of traditional carbon fibers are improved at the same time, that is, the thermal conductivity of graphene fibers far exceeds that of traditional carbon fibers, but its modulus is lower than that of traditional carbon fibers.
  • High thermal conductivity and high modulus are two key indicators for simultaneous improvement in traditional carbon fibers, and are usually closely related to the degree of orientation and density of fibers.
  • the orientation degree of graphene fibers can reach more than 90%.
  • graphene fibers are directly assembled from single-layer graphene. Ultimately determines the density of graphene fibers, so improving the order of the two-dimensional graphene sheet arrangement in graphene fibers will improve the density of graphene fibers, thereby preparing graphene fibers with high modulus and high thermal conductivity.
  • the present invention provides an airgel fiber with specific cross-sectional morphology and its preparation method and device, and obtains a graphene fiber with high modulus and high thermal conductivity.
  • This application is aimed at two-dimensional planar nanosheets. Based on the unique huge aspect ratio of two-dimensional planar nanosheets, it has a good lyotropic liquid crystal phenomenon; based on the unique macromolecules of two-dimensional planar nanosheets, it has the dynamic stability of liquid crystals.
  • a hydrogel fiber with a specific structure is formed. After the gel fiber is freeze-dried, an airgel fiber with a specific cross-sectional shape is obtained.
  • the primary graphene oxide fibers can be obtained after the hydrogel fibers are dried and densified, and the graphene oxide fibers with high modulus and high thermal conductivity can be obtained by plasticizing and stretching, chemical reduction and heat treatment. .
  • the airgel fiber with specific cross-sectional shape characteristics of the present invention is composed of two-dimensional nanosheets, and the fiber cross-section is arranged in concentric circular sheets or radial helical sheets.
  • the preparation method of the above-mentioned airgel fiber is: extruding the dispersion liquid of the two-dimensional nanosheet into the coagulation bath, and then fixing the structure after solidification to obtain the airgel fiber with specific cross-sectional shape characteristics; the extrusion speed includes The axial speed in the out direction and the circumferential rotational speed perpendicular to the axial speed.
  • circumferential velocity is brought about by introducing circumferential rotational shear force into the dispersion of two-dimensional nanosheets.
  • the two-dimensional nanosheets are graphene oxide, graphene, Mxene, molybdenum disulfide, montmorillonite nanosheets with two-dimensional anisotropy and various mixed two-dimensional nanosheets.
  • the concentration of the dispersion of the two-dimensional nanosheets is greater than 1 mg/g.
  • the present invention also relates to a device for preparing airgel fibers with specific cross-sectional morphological characteristics, at least including an extruding device, a coagulation bath and a freeze-drying system; the extruding device includes a spinning tube, and the spinning There is a circumferential rotational shear force inside the tube.
  • the rotor is located at the axial center of the spinning tube.
  • the rotor in the spinning tube rotates along its axis.
  • the present invention also provides a graphene fiber with high modulus and high thermal conductivity, which is composed of graphene two-dimensional nanosheets, and the cross section of the fiber is arranged in concentric circular sheets, and the two-dimensional graphene nanosheets are arranged along the axial direction.
  • the graphene sheets constitute a plurality of graphite crystals with an axial length of more than 200nm and a radial length of more than 100nm; the graphene fiber density is greater than or equal to 1.9g/cm 3 .
  • the present invention also relates to the preparation method of the above-mentioned graphene fiber, the method is: extruding the dispersion liquid of the graphene oxide two-dimensional nanosheet into the coagulation bath, and obtaining the nascent graphene oxide fiber after drying; Stretching, chemical reduction and heat treatment to obtain graphene fibers with high modulus and high thermal conductivity; wherein, the extrusion speed includes the axial speed along the extrusion direction and the circumferential rotational speed perpendicular to the axial speed.
  • circumferential velocity is brought about by introducing circumferential rotational shear force into the dispersion of two-dimensional nanosheets.
  • the dispersion of the graphene oxide two-dimensional nanosheets is an aqueous phase dispersion of graphene oxide, a DMF phase dispersion, a DMAc phase dispersion, a DMSO phase dispersion, and the coagulation bath is ethyl acetate, dichloromethane , acetic acid, ethanol, isopropanol, chloroform, acetone, etc. and their mixed coagulation baths, or aqueous coagulation baths of high-valence salts, and the high-valence salts are calcium chloride, ferrous chloride or ferric sulfate.
  • plasticizing and stretching refers to: stretching the fiber by immersing it in a plasticizer
  • the plasticizer is selected from: glycerol, propylene glycol, ethylene glycol, triethylene glycol, acetone, isopropanol , acetic acid, methanol, tetraethylene glycol, pentaethylene glycol, hydrochloric acid, dilute sulfuric acid, organic amines, etc. or their mixed plasticizers.
  • the reagents used in the chemical reduction are hydroiodic acid, hydrazine hydrate, sodium ascorbate, stannous chloride, etc., and the heat treatment temperature is 1300-3000 degrees Celsius.
  • the present invention also provides the application of the above fiber in sensing, phase change energy storage, and catalytic energy.
  • airgel fibers with specific cross-sectional morphological characteristics can be prepared, which solves the problem that the two-dimensional nanosheets inside the airgel fiber cannot be precisely adjusted for sheet arrangement, thereby Improve the mechanical properties and conductivity of airgel fibers, and promote the practical application of airgel fibers.
  • the present invention improves the orderliness of the graphene sheet arrangement inside the fiber by constructing a graphene fiber structure with a specific structure, thereby improving the density of the final heat-treated graphene fiber, so that the crystallinity of graphene during heat treatment is significantly improved, and the crystal The size is significantly increased, which greatly improves the thermal conductivity and modulus of graphene fibers.
  • Figure 1 is a schematic diagram of a self-made rotary extrusion spinning device.
  • Figure 2 shows the rotor structure in the rotary extrusion device.
  • Figure 3 shows the cross-sectional morphology of graphene oxide airgel fibers prepared at different graphene liquid crystal spinning liquid concentrations and different rotor speeds.
  • Figure 4 shows the cross-sectional shapes of three typical graphene oxide airgel fibers, including a is a random distribution cross-sectional structure; b is a concentric cross-sectional structure; c is a helical cross-sectional structure.
  • Figure 5 is the mechanical curve of graphene fibers.
  • Concentric GF is the graphene fiber after coagulation, drying and heat treatment of gel fibers distributed in concentric circles; Random GF is graphene after coagulation, drying and heat treatment of gel fibers distributed randomly fiber.
  • the cross-sectional morphology of the prepared graphene oxide airgel fibers is shown in Fig. 4a.
  • the cross-sectional morphology of the prepared graphene oxide airgel fibers is shown in Figure 4b. This is because graphene oxide is a kind of macromolecule, and liquid crystal has good dynamic stability, so that its specific structure can be maintained after passing through the rotating flow field, and finally the arrangement structure of graphene macromolecules after passing through the rotating flow field It is continued to graphene oxide airgel fibers and corresponding graphene airgel fibers.
  • the cross-sectional shape of the airgel fiber is mainly determined by the concentration of the graphene oxide liquid crystal spinning solution and the rotor speed.
  • the concentration of the graphene oxide solution determines whether it can form liquid crystals.
  • the concentration of the graphene oxide solution is above 0.1 wt% to form liquid crystals.
  • the rotor speed increases, and the cross-section of the graphene oxide airgel fiber first assumes a concentric circle structure, and when the speed is further increased, the fiber cross-section presents a helical structure.
  • Regulating the graphene oxide concentration to form liquid crystals is common knowledge in the art, and those skilled in the art can regulate the cross-sectional morphology of the gel fiber according to the above-mentioned law of rotational speed.
  • the prepared heat-treated graphene airgel fiber After testing, the prepared heat-treated graphene airgel fiber has a higher thermal conductivity, reaching 15W/(m K), in contrast, the thermal conductivity of the disorderly arranged graphene airgel fiber is only insufficient. 10W/(m K), high thermal conductivity graphene airgel fiber framework can be used for thermal, electrical, and photoresponsive functional materials.
  • the dried graphene oxide fibers are subjected to chemical reduction of hydroiodic acid and heat treatment at 2700 degrees to obtain graphene fibers with high modulus and high thermal conductivity.
  • the graphene fiber prepared from the concentric gel fiber has a strength of 3GPa, a modulus of 833GPa, and a thermal conductivity of 1590W/(m K).
  • the mechanical curve is shown in Figure 5 Concentric GF.
  • the dried graphene oxide fibers are subjected to chemical reduction of hydroiodic acid and heat treatment at 2700 degrees to obtain graphene fibers prepared from randomly distributed gel fibers.
  • the graphene fiber without microfibrillation has a strength of 3.1GPa, a modulus of 343GPa, and a thermal conductivity of 1400W/(m K).
  • the mechanical curve is shown in Figure 5Random GF.
  • the dried graphene oxide fiber is subjected to chemical reduction of hydroiodic acid and heat treatment at 2700 degrees to obtain the final graphene fiber.
  • the graphene fiber prepared under this condition has a strength of 2GPa, a modulus of 650GPa, and a thermal conductivity of 1490W/(m K).
  • This comparative example is the same as the embodiment 8, the difference is that: the rotating speed of the rotor is 500rpm, forming a helical structure.
  • the dried graphene oxide fiber is subjected to chemical reduction of hydroiodic acid and heat treatment at 2700 degrees to obtain the final graphene fiber.
  • the graphene fiber prepared under this condition has a strength of 1.8GPa, a modulus of 500GPa, and a thermal conductivity of 1360W/(m K).

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Fibers (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention concerne une fibre d'aérogel présentant une caractéristique morphologique de section spécifique, un procédé et un dispositif de préparation associés. La forme d'agencement des nanofeuillets bidimensionnels sur la section de la fibre aérogel est réglable. Un procédé de régulation est le suivant : pendant le filage humide, ajout d'un dispositif de champ d'écoulement rotatif avant la pulvérisation d'un fluide de solution de filage, le champ d'écoulement rotatif faisant en sorte que les nanofeuillets bidimensionnels forment un agencement de couche de feuille spécifique dans une direction de section d'une fibre de gel sous l'action d'un cisaillement rotatif ; et préparation d'une fibre d'aérogel d'oxyde de graphène d'une structure morphologique spécifique (un cercle concentrique et une ligne hélicoïdale) à partir de la fibre de gel d'une structure de section morphologique spécifique dans des conditions de lyophilisation. Une fibre d'hydrogel à structure en cercle concentrique est soumise à une densification par séchage, un étirage et une réduction pour obtenir une fibre de graphène avec un module élevé et une conductivité thermique élevée ; par rapport aux fibres de graphène existantes, la conductivité thermique et le module de la fibre de graphène obtenue sont améliorés.
PCT/CN2021/137642 2021-12-14 2021-12-14 Fibre d'aérogel présentant une caractéristique morphologique de section spécifique, procédé et dispositif de préparation associés WO2023108378A1 (fr)

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PCT/CN2021/137642 WO2023108378A1 (fr) 2021-12-14 2021-12-14 Fibre d'aérogel présentant une caractéristique morphologique de section spécifique, procédé et dispositif de préparation associés
JP2023574187A JP2024520603A (ja) 2021-12-14 2021-12-14 特定断面形態特徴を有するエアロゲル繊維、これを製造する方法及び装置と、グラフェン繊維及びこれを製造する方法と、これら繊維の応用
US18/434,741 US20240175169A1 (en) 2021-12-14 2024-02-06 Aerogel fiber having specific cross-sectional morphological feature, graphene fiber and preparation method and device therefor

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PCT/CN2021/137642 WO2023108378A1 (fr) 2021-12-14 2021-12-14 Fibre d'aérogel présentant une caractéristique morphologique de section spécifique, procédé et dispositif de préparation associés

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101049991A (zh) * 2007-05-09 2007-10-10 山东大学 一种纳米TiO2纤维套筒的制备方法
CN103726133A (zh) * 2014-01-02 2014-04-16 东华大学 高强度、紧凑有序多孔石墨烯纤维及其连续制备方法
CN103806128A (zh) * 2014-01-15 2014-05-21 北京理工大学 一种氧化石墨烯纤维及其制备方法和应用
US20140308449A1 (en) * 2013-04-15 2014-10-16 Aruna Zhamu Process for producing continuous graphitic fibers from living graphene molecules
CN106183142A (zh) * 2016-07-18 2016-12-07 浙江大学 一种基于石墨烯纤维无纺布的自热膜
CN110117839A (zh) * 2019-05-22 2019-08-13 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 螺旋形TiO2/石墨烯复合纤维、其制备方法及应用
CN111676591A (zh) * 2020-06-11 2020-09-18 南京信息工程大学 一种氧化石墨烯气凝胶纤维织物及其制备方法与应用

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101049991A (zh) * 2007-05-09 2007-10-10 山东大学 一种纳米TiO2纤维套筒的制备方法
US20140308449A1 (en) * 2013-04-15 2014-10-16 Aruna Zhamu Process for producing continuous graphitic fibers from living graphene molecules
CN103726133A (zh) * 2014-01-02 2014-04-16 东华大学 高强度、紧凑有序多孔石墨烯纤维及其连续制备方法
CN103806128A (zh) * 2014-01-15 2014-05-21 北京理工大学 一种氧化石墨烯纤维及其制备方法和应用
CN106183142A (zh) * 2016-07-18 2016-12-07 浙江大学 一种基于石墨烯纤维无纺布的自热膜
CN110117839A (zh) * 2019-05-22 2019-08-13 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 螺旋形TiO2/石墨烯复合纤维、其制备方法及应用
CN111676591A (zh) * 2020-06-11 2020-09-18 南京信息工程大学 一种氧化石墨烯气凝胶纤维织物及其制备方法与应用

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